HRID466220

反应详情

EQUATION

反应方程式

HRID 466220 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A solution of 4-hydroxy benzonitrile (55 g) in methanol (100 ml) was treated with potassium hydroxide (29 g) in water (30 ml) and evaporated at reduced pressure. The remaining potassium salt was dissolved in dry dimethylformamide (75 ml) and (4R)-2,2-dimethyl-4 - methanesulfonyloxymethyl-1,3-dioxolane, 82.2 g, was add stirring at 110° C. for 20 h, allowed to cool and distributed between ether and water. The aqueous phase was extracted three times with ether, the combined ether phases washed three times with 10% aqueous potassium hydroxide and twice with water, dried over anhydrous sodium sulfate and evaporated. Yield 77 g of the title compound.

WORKUP

后处理

  1. customevaporated at reduced pressure
  2. dissolutionThe remaining potassium salt was dissolved in dry dimethylformamide (75 ml)
  3. addition(4R)-2,2-dimethyl-4 - methanesulfonyloxymethyl-1,3-dioxolane, 82.2 g, was add
  4. temperatureto cool
  5. extractionThe aqueous phase was extracted three times with ether
  6. washthe combined ether phases washed three times with 10% aqueous potassium hydroxide
  7. dry with materialtwice with water, dried over anhydrous sodium sulfate
  8. customevaporated